阻燃型木纤维—聚丙烯复合材料制备及性能研究
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摘要
木塑复合材料是当前生物质材料研究领域中重要的研究方向之一。但是，由于木塑复合材料属于易燃材料，直接用于室内存在一定的安全隐患。本文开展的阻燃型木纤维-聚丙烯复合材料的研究，将提供一种具有阻燃功能的新型木塑复合材料，为扩展木塑复合材料的室内应用提供技术基础。
在本研究中，木纤维-聚丙烯复合材料的制备采用人造板平压工艺。通过对复合材料物理力学性能、燃烧性能等主要影响因子的研究，利用热重-差热联用分析仪、锥形量热仪以及红外光谱分析仪在对原料及复合材料的热解、燃烧特性进行分析基础上，筛选出适当的阻燃剂体系。在进行工艺因子与阻燃型木塑复合材料性能的相关性分析评价后，制备出高性能的阻燃型木塑复合材料。
本论文的主要研究结果如下：
1．聚丙烯(PP)加量、补强剂种类、产品密度和纤维形态四个变量因子对复合材料的物理力学性能有不同程度的影响。增加PP用量复合材料的各项物理力学性能都有显著提高；补强剂对复合材料物理力学性能提高也较明显，以2％PAPI的效果更好；提高产品密度对抗弯性能提高最显著；纤维形态对产品性能的影响规律不明显。制备高性能的木纤维-聚丙烯复合材料最佳因子水平为：PP加量为40％，补强剂为2％PAPI，产品密度为1.05g／cm~3，纤维形态为中粗纤维，制备的复合材料性能大幅度超过GB／T11718-1999室外用纤维板要求。
2．塑料原料的燃烧热是决定木塑复合材料燃烧性能的关键因子。PP燃烧热值高，其加量对复合材料的滞燃性能有非常显著的负面影响。复合材料中PP含量增加，复合材料氧指数大幅度降低，热释放速率和燃烧热值迅速升高。加入补强剂加速了复合材料的燃烧过程；其他因素如产品密度和纤维形态对复合材料的燃烧特性影响规律不明显。木塑复合材料的热解过程中，木纤维和聚丙烯有相互促进热解、燃烧的现象。
3．通过改变木纤维热解方式，SA阻燃剂促进木纤维提前分解成炭，减缓燃烧过程达到阻燃目的。通过热解活化能计算、红外光谱分析等机理分析证实，阻燃剂SA对木材的脱水过程中促使木材纤维表面活化，促使木塑界面和纤维间更好的相互融合，进而提高了木塑复合材料的物理力学性能，这一结论与传统的阻燃型人造板制造中阻燃剂对板材性能起负面作用的结论相反。
塑料阻燃剂以质量比3∶1的十溴二苯乙烷和三氧化二锑组成的DBT配方，质量比2.7∶1的十溴二苯乙烷和硼酸锌组成的DBZ配方以及100％高聚磷酸铵的APM配方阻燃效果较好。
由于阻燃剂阻燃机理的不同，单独使用木纤维阻燃剂或塑料阻燃剂配方都难以达到对木塑复合材料既定的阻燃目标。
4．制备阻燃型木纤维-聚丙烯复合材料的结果表明：木纤维阻燃剂SA加量、补强剂种类、补强剂加量、塑料阻燃剂种类、塑料阻燃剂加量和木塑比例6个变量因子中，木材阻燃剂SA加量、塑料阻燃剂加量和木塑比例对木塑复合材料的阻燃性能(氧指数)有显著影响，其他因子影响不显著。木材阻燃剂SA加入不仅显著提高了板材的氧指数，还使板材的一些物理力学性能有了显著提高；塑料阻燃剂APM和木材阻燃剂SA共同作用使木塑复合材料的阻燃效果显著增加；PP塑料在复合材料中含量的提高可以显著增强复合材料的物理力学性能，但导致材料氧指数有较大幅度的降低；补强剂加量增加可有效提高复合材料物理力学性能，而补强剂种类和塑料阻燃剂种类对物理力学性能的影响较小。木纤维阻燃剂SA影响了补强剂的固化效果，其交互作用对物理力学性能有一定的影响。
与普通木塑复合材料相比，阻燃型木塑复合材料氧指数显著提高，在整个燃烧过程的热释放速率，平均质量损失速率和有效燃烧热值等燃烧特性值都有显著降低。
在最优工艺条件下，本研究制备的阻燃型木塑复合材料性能达到以下指标：氧指数为39.6％，达到国家公共安全行业标准GA87-94中防火板F1级中氧指数≥35％的要求；物理力学性能：24h吸水厚度膨胀率为10.18％，内结合强度为0.966MPa，静曲强度为35.45MPa，弹性模量为4031MPa，沸腾试验内结合强度为0.272MPa，超过GB／T11718-1999中室内潮湿环境用(防潮型)中密度纤维板要求，甚至达到室外用板的性能指标。研究达到预期目标。
Research on wood-plastic composites is one of important part in the filed of biomaterials science.As flammability character of wood-plastic composites,fire hazard exists for its indoor usage.The main objective of this study is to find out new flame-retardant wood-plastic composites that can be used indoors and collect technical data for study in its further indoor application.
In the experiment,wood fiber-polypropylene (PP) composites were made by manufacturing process of wood-based board.The main experimental factors that influence physical-mechanical properties and combustion properties of wood fiber-PP composites was analyzed first,then proper fire retardants were chosen for wood fiber-PP composites by utilizing these data from TG-DTA analysis,cone calorimeter and FTIR analysis.Finally orthogonal experimental design method was used to analyze the relations among key factors and properties of fire retardant composites.By the experiment result,a kind of flame-retardant wood fiber-PP composites with excellent physical-mechanical properties was produced.
In this paper,the main research conclusions are as follows.
1.PP content,reinforcement species,density of products and fiber size were considered as experimental factors and their influence on physical-mechanical properties of wood fiber-PP composites was analyzed.The results showed that the four factors had different effect on physical-mechanical properties.More PP content caused significant enhancement of physical-mechanical properties;reinforcement can increase the properties very well,especially when adding 2％PAPI in the composites;When the designed density increased,it caused the most significant improvement on properties of modulus of rupture (MOR) and modulus of elasticity (MOE);Influence of fiber size on properties is not significant,but middle-size fiber had relatively better performance.As a result,to produce excellent wood fiber-PP composites,the levels of factors should be:40％PP content,2％PAPI,1.05g/cm~3 density and middle size fiber.Test results showed that composites made under the chosen factors had super properties and could meet requirement of national standard GB/T11718-1999 for exterior fiberboard.
2.The crucial factor dominating combustion properties of composites was combustion heat of PP material.Combustion heat of PP was much higher than wood and it badly decreased fire endurance of composites. With the increase of PP,the oxygen index (OI) fell down,heat release rate (HRR) and effective heat of combustion (EHC) increased rapidly.Reinforcement kept dimensional stability in fire but accelerated burring behavior of composites;other variables,such as density of product and fiber size had some effect on fire behavior,but their influence was not significant.The calculated apparent activation energy showed that in the pyrolysis process of wood and PP composites,the materials showed co-decomposition behavior.
3.TG and DTA analysis results showed that SA changed thermal pyrolysis characteristics of wood.Flame-retardance resulted from SA catalyzing decomposition of wood to charcoal at lower temperature to slower combustion process.The test results of physical-mechanical properties showed that differ from regular fire-retardant wood-based panels,the SA fire retardant enhanced physical-mechanical properties of wood fiber-PP composites.It can be explained like that SA enhanced surface activation of wood fiber and that could make activated bonding at interface of wood and PP and was identified in mechanism analysis.
Different ratio of plastic fire retardant led to different OI of PP.Following three kind of compound have good performance on flame retardance:DBT compound by 3 parts of decabromodiphenyl ethane (DBDPE) and 1 part of antimony trioxide (ST);DBZ compound by 2.7 parts of DBDPE and 1 part of zinc borate (ZB),APM made from 100％ammonium polyphosphate (APP).
Because of different fire retarding mechanism,using wood fiber fire retardant or plastic fire retardant alone can not meet fire retardant objective of wood fiber-PP composites.
4.Six experimental variables,such as SA content,reinforcement species,reinforcement content,plastic fire retardant species (PFRS, plastic fire retardant content (PFRC) and ratio between wood fiber and PP (WPR) were tested in manufacturing fire-retardant wood-plastic composites.The results showed that the SA content,PFRC and WPR were significant factors for fire retardant effect (OI) and other factors were not very important.Increase of SA content not only improved OI of composites,but also improved some physical-mechanical properties greatly;cooperation of APP in APM prescription and SA fire retardant made flameproof property improved significantly;adding PP can increase physical-mechanical properties at large scale but decrease OI rapidly.Reinforcement can increase the properties greatly,but reinforcement species and PWFS were not significant compared with other factors.Properties of SA had some bad effect on cure degree of reinforcement;their interaction had some influence on physical-mechanical properties of composites.
Compared with normal wood fiber-PP composites,fire-retardant wood fiber-PP composites had much higher OI,and heat release rate (HRR),mean mass loss rate (MMLR) and mean effective heat of combustion (MEHC) was slow down greatly.
Using the optimized factors the properties of fire-retardant wood fiber-PP composites were excellent.OI was 39.6％,which meet requirements of OI≥35％in standard GA87-94;thickness swelling after 24hour water absorption (24hTS) was 10.18％,internal bond (IB) was 0.966MPa,modulus of rupture (MOR) was 35.45MPa, modulus of elasticity (MOE) was 4031MPa and boiling test of internal bond (BTIB) was 0.272MPa. The test result surpassed national requirements of GB/Tl1718-1999 of humid resistant fiberboard, and it even meet requirement for outdoor usage.Objectives of the research had been met.
在本研究中，木纤维-聚丙烯复合材料的制备采用人造板平压工艺。通过对复合材料物理力学性能、燃烧性能等主要影响因子的研究，利用热重-差热联用分析仪、锥形量热仪以及红外光谱分析仪在对原料及复合材料的热解、燃烧特性进行分析基础上，筛选出适当的阻燃剂体系。在进行工艺因子与阻燃型木塑复合材料性能的相关性分析评价后，制备出高性能的阻燃型木塑复合材料。
本论文的主要研究结果如下：
1．聚丙烯(PP)加量、补强剂种类、产品密度和纤维形态四个变量因子对复合材料的物理力学性能有不同程度的影响。增加PP用量复合材料的各项物理力学性能都有显著提高；补强剂对复合材料物理力学性能提高也较明显，以2％PAPI的效果更好；提高产品密度对抗弯性能提高最显著；纤维形态对产品性能的影响规律不明显。制备高性能的木纤维-聚丙烯复合材料最佳因子水平为：PP加量为40％，补强剂为2％PAPI，产品密度为1.05g／cm~3，纤维形态为中粗纤维，制备的复合材料性能大幅度超过GB／T11718-1999室外用纤维板要求。
2．塑料原料的燃烧热是决定木塑复合材料燃烧性能的关键因子。PP燃烧热值高，其加量对复合材料的滞燃性能有非常显著的负面影响。复合材料中PP含量增加，复合材料氧指数大幅度降低，热释放速率和燃烧热值迅速升高。加入补强剂加速了复合材料的燃烧过程；其他因素如产品密度和纤维形态对复合材料的燃烧特性影响规律不明显。木塑复合材料的热解过程中，木纤维和聚丙烯有相互促进热解、燃烧的现象。
3．通过改变木纤维热解方式，SA阻燃剂促进木纤维提前分解成炭，减缓燃烧过程达到阻燃目的。通过热解活化能计算、红外光谱分析等机理分析证实，阻燃剂SA对木材的脱水过程中促使木材纤维表面活化，促使木塑界面和纤维间更好的相互融合，进而提高了木塑复合材料的物理力学性能，这一结论与传统的阻燃型人造板制造中阻燃剂对板材性能起负面作用的结论相反。
塑料阻燃剂以质量比3∶1的十溴二苯乙烷和三氧化二锑组成的DBT配方，质量比2.7∶1的十溴二苯乙烷和硼酸锌组成的DBZ配方以及100％高聚磷酸铵的APM配方阻燃效果较好。
由于阻燃剂阻燃机理的不同，单独使用木纤维阻燃剂或塑料阻燃剂配方都难以达到对木塑复合材料既定的阻燃目标。
4．制备阻燃型木纤维-聚丙烯复合材料的结果表明：木纤维阻燃剂SA加量、补强剂种类、补强剂加量、塑料阻燃剂种类、塑料阻燃剂加量和木塑比例6个变量因子中，木材阻燃剂SA加量、塑料阻燃剂加量和木塑比例对木塑复合材料的阻燃性能(氧指数)有显著影响，其他因子影响不显著。木材阻燃剂SA加入不仅显著提高了板材的氧指数，还使板材的一些物理力学性能有了显著提高；塑料阻燃剂APM和木材阻燃剂SA共同作用使木塑复合材料的阻燃效果显著增加；PP塑料在复合材料中含量的提高可以显著增强复合材料的物理力学性能，但导致材料氧指数有较大幅度的降低；补强剂加量增加可有效提高复合材料物理力学性能，而补强剂种类和塑料阻燃剂种类对物理力学性能的影响较小。木纤维阻燃剂SA影响了补强剂的固化效果，其交互作用对物理力学性能有一定的影响。
与普通木塑复合材料相比，阻燃型木塑复合材料氧指数显著提高，在整个燃烧过程的热释放速率，平均质量损失速率和有效燃烧热值等燃烧特性值都有显著降低。
在最优工艺条件下，本研究制备的阻燃型木塑复合材料性能达到以下指标：氧指数为39.6％，达到国家公共安全行业标准GA87-94中防火板F1级中氧指数≥35％的要求；物理力学性能：24h吸水厚度膨胀率为10.18％，内结合强度为0.966MPa，静曲强度为35.45MPa，弹性模量为4031MPa，沸腾试验内结合强度为0.272MPa，超过GB／T11718-1999中室内潮湿环境用(防潮型)中密度纤维板要求，甚至达到室外用板的性能指标。研究达到预期目标。
Research on wood-plastic composites is one of important part in the filed of biomaterials science.As flammability character of wood-plastic composites,fire hazard exists for its indoor usage.The main objective of this study is to find out new flame-retardant wood-plastic composites that can be used indoors and collect technical data for study in its further indoor application.
In the experiment,wood fiber-polypropylene (PP) composites were made by manufacturing process of wood-based board.The main experimental factors that influence physical-mechanical properties and combustion properties of wood fiber-PP composites was analyzed first,then proper fire retardants were chosen for wood fiber-PP composites by utilizing these data from TG-DTA analysis,cone calorimeter and FTIR analysis.Finally orthogonal experimental design method was used to analyze the relations among key factors and properties of fire retardant composites.By the experiment result,a kind of flame-retardant wood fiber-PP composites with excellent physical-mechanical properties was produced.
In this paper,the main research conclusions are as follows.
1.PP content,reinforcement species,density of products and fiber size were considered as experimental factors and their influence on physical-mechanical properties of wood fiber-PP composites was analyzed.The results showed that the four factors had different effect on physical-mechanical properties.More PP content caused significant enhancement of physical-mechanical properties;reinforcement can increase the properties very well,especially when adding 2％PAPI in the composites;When the designed density increased,it caused the most significant improvement on properties of modulus of rupture (MOR) and modulus of elasticity (MOE);Influence of fiber size on properties is not significant,but middle-size fiber had relatively better performance.As a result,to produce excellent wood fiber-PP composites,the levels of factors should be:40％PP content,2％PAPI,1.05g/cm~3 density and middle size fiber.Test results showed that composites made under the chosen factors had super properties and could meet requirement of national standard GB/T11718-1999 for exterior fiberboard.
2.The crucial factor dominating combustion properties of composites was combustion heat of PP material.Combustion heat of PP was much higher than wood and it badly decreased fire endurance of composites. With the increase of PP,the oxygen index (OI) fell down,heat release rate (HRR) and effective heat of combustion (EHC) increased rapidly.Reinforcement kept dimensional stability in fire but accelerated burring behavior of composites;other variables,such as density of product and fiber size had some effect on fire behavior,but their influence was not significant.The calculated apparent activation energy showed that in the pyrolysis process of wood and PP composites,the materials showed co-decomposition behavior.
3.TG and DTA analysis results showed that SA changed thermal pyrolysis characteristics of wood.Flame-retardance resulted from SA catalyzing decomposition of wood to charcoal at lower temperature to slower combustion process.The test results of physical-mechanical properties showed that differ from regular fire-retardant wood-based panels,the SA fire retardant enhanced physical-mechanical properties of wood fiber-PP composites.It can be explained like that SA enhanced surface activation of wood fiber and that could make activated bonding at interface of wood and PP and was identified in mechanism analysis.
Different ratio of plastic fire retardant led to different OI of PP.Following three kind of compound have good performance on flame retardance:DBT compound by 3 parts of decabromodiphenyl ethane (DBDPE) and 1 part of antimony trioxide (ST);DBZ compound by 2.7 parts of DBDPE and 1 part of zinc borate (ZB),APM made from 100％ammonium polyphosphate (APP).
Because of different fire retarding mechanism,using wood fiber fire retardant or plastic fire retardant alone can not meet fire retardant objective of wood fiber-PP composites.
4.Six experimental variables,such as SA content,reinforcement species,reinforcement content,plastic fire retardant species (PFRS, plastic fire retardant content (PFRC) and ratio between wood fiber and PP (WPR) were tested in manufacturing fire-retardant wood-plastic composites.The results showed that the SA content,PFRC and WPR were significant factors for fire retardant effect (OI) and other factors were not very important.Increase of SA content not only improved OI of composites,but also improved some physical-mechanical properties greatly;cooperation of APP in APM prescription and SA fire retardant made flameproof property improved significantly;adding PP can increase physical-mechanical properties at large scale but decrease OI rapidly.Reinforcement can increase the properties greatly,but reinforcement species and PWFS were not significant compared with other factors.Properties of SA had some bad effect on cure degree of reinforcement;their interaction had some influence on physical-mechanical properties of composites.
Compared with normal wood fiber-PP composites,fire-retardant wood fiber-PP composites had much higher OI,and heat release rate (HRR),mean mass loss rate (MMLR) and mean effective heat of combustion (MEHC) was slow down greatly.
Using the optimized factors the properties of fire-retardant wood fiber-PP composites were excellent.OI was 39.6％,which meet requirements of OI≥35％in standard GA87-94;thickness swelling after 24hour water absorption (24hTS) was 10.18％,internal bond (IB) was 0.966MPa,modulus of rupture (MOR) was 35.45MPa, modulus of elasticity (MOE) was 4031MPa and boiling test of internal bond (BTIB) was 0.272MPa. The test result surpassed national requirements of GB/Tl1718-1999 of humid resistant fiberboard, and it even meet requirement for outdoor usage.Objectives of the research had been met.
引文
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